CN107913304A - Dripping pill containing Prunella vulgaris extract and preparation method thereof - Google Patents
Dripping pill containing Prunella vulgaris extract and preparation method thereof Download PDFInfo
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- CN107913304A CN107913304A CN201610884490.5A CN201610884490A CN107913304A CN 107913304 A CN107913304 A CN 107913304A CN 201610884490 A CN201610884490 A CN 201610884490A CN 107913304 A CN107913304 A CN 107913304A
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- eluent
- selfheal
- eluant
- water
- prunella vulgaris
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
- A61K36/536—Prunella or Brunella (selfheal)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/0012—Galenical forms characterised by the site of application
- A61K9/0053—Mouth and digestive tract, i.e. intraoral and peroral administration
- A61K9/006—Oral mucosa, e.g. mucoadhesive forms, sublingual droplets; Buccal patches or films; Buccal sprays
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2022—Organic macromolecular compounds
- A61K9/2031—Organic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyethylene glycol, polyethylene oxide, poloxamers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Abstract
The invention discloses a kind of dripping pill containing Prunella vulgaris extract, it includes Prunella vulgaris extract and matrix；The Prunella vulgaris extract obtains as follows：Selfheal is extracted as Extraction solvent by the use of water or ethanol water, obtains selfheal crude extract；By macroporous resin column on the selfheal crude extract, gradient elution is carried out using the ethanol water of water, the ethanol water of 10~30vol% and 50~95vol% successively；Eluent after the ethanol water of 50~95vol% is eluted concentrates, dry, to obtain the final product.The dripping pill containing Prunella vulgaris extract of the present invention has significant prevention and treatment insomnia effect.
Description
Technical field
The present invention relates to a kind of dripping pill with sedative-hypnotic effect, the particularly dripping pill containing Prunella vulgaris extract, also relate to
And the preparation method of the dripping pill.
Background technology
Insomnia refers to that patient is unsatisfactory for the length of one's sleep and (or) quality and influences a kind of subjective body of social function in the daytime
Test.Clinically for the means of intervention of insomnia, it is divided into non-drug therapy and drug therapy.Drug therapy based on Western medicine, but
The main application of most drugs be not treatment insomnia, long-term use of hypnotic it is possible that drowsiness, forgetful, allergy etc. no
Good reaction, or even tolerance, additive etc. are produced, insomnia is aggravated, induces depression etc..People increasingly pay attention to Chinese medicine pair
The therapeutic effect of insomnia.
Title is insomnia, must not sleep in traditional Chinese medicine, mesh does not set for insomnia, must not crouch, sleeping uneasiness etc. of sleeping.It is insomnia former, or because of heresy
Gas is disturbed, or is stagnation of phlegm and QI, or the moon does not contain sun, or conscience fire is disturbed." though non-one kind, caused by always sun does not hand over the moon ", therefore, wish to get
Reposal, must hand over its negative and positive, or dispel its evil or disappear its phlegm or its foster the moon, or its clear heat.Selfheal reports the body of the moon, assigns sun and is used.
Ming Dynasty's Wang Kentang《Clever orchid guide》(1602), described in book：" Chinese toon field often with the tuber of pinellia processed, each five money of selfheal, takes yin-yang match
Justice, dense pan-fried running water, unexpectedly inflammatory blepharoedema and crouch." just Given this mechanism, medical field is on the tuber of pinellia and the prescription of selfheal compatibility composition
The research for the treatment of insomnia is more, and the report individually using selfheal treatment insomnia is less.Chinese patent literature
CN101507751A discloses purposes of the Prunella vulgaris extract in medicament for treating insomnia is prepared, it is found that selfheal carries through ethanol
Take, then there is obvious calm, hypnotic activity with the Prunella vulgaris extract obtained after petroleum ether degreasing.The document thinks that the summer is withered
The component with sedative-hypnotic effect is the component that polarity is larger in alcohol extracting thing in grass, thus eliminates low pole using petroleum ether
Property component.The document is also without the preparation of open Prunella vulgaris extract.
Therefore, it is necessary to the selfheal Chinese medicine preparation that a kind of simple and effective, suitable for clinical expansion treatment is had a sleepless night.
The content of the invention
The inventors of the present application found that using Prunella vulgaris extract made from ad hoc approach, there is splendid tranquilizing soporific
Effect, is adapted to treatment insomnia；Further study show that the treatment insomnia of the dropping pill formulation of Prunella vulgaris extract is better,
It is significantly better than other formulations.
It is an object of the invention to provide a kind of selfheal dripping pill, which contains Prunella vulgaris extract, it is withered to combine the summer
The effect of careless extract and the advantage of formulation, have that dissolving is fast, absorbs advantage fast, that effect is fast, bioavilability is high, for clinic
Treatment insomnia provides a kind of simple, effective, cheap Chinese medicine preparation.
Another object of the present invention is to provide the preparation method of the selfheal dripping pill.
The purpose of the present invention is what is be achieved through the following technical solutions：
The present invention provides a kind of dripping pill containing Prunella vulgaris extract, including Prunella vulgaris extract and matrix；Wherein, the summer
Withered grass extract obtains as follows：
(1) selfheal is extracted as Extraction solvent by the use of water or ethanol water, obtains selfheal crude extract, the ethanol water
Concentration of alcohol in solution is 20~95vol%；
(2) the selfheal crude extract is placed in macroporous resin column, successively using the first eluant, eluent, the second eluant, eluent and
Three eluant, eluents carry out gradient elution, collect the eluent after the 3rd eluent；First eluant, eluent is water, described second
Eluant, eluent is the ethanol water that concentration of alcohol is 10~30vol%, the 3rd eluant, eluent is concentration of alcohol for 50~
The ethanol water of 95vol%；
(3) by eluent concentration, the drying after the 3rd eluent, Prunella vulgaris extract is obtained.
In the step (1) of the present invention, by the use of water or ethanol water as solvent extraction selfheal, extracting solution is concentrated,
Through being further dried or not after drying, obtaining the selfheal crude extract.A kind of embodiment according to the present invention, extraction are molten
Agent is water, and extracting solution is concentrated into certain volume, without drying, obtains selfheal crude extract, the selfheal crude extract of the liquid
It is directly entered elution step.A kind of preferred embodiment according to the present invention, Extraction solvent is water, and extracting solution is concentrated, is done
It is dry, obtain selfheal crude extract.Another preferred embodiment according to the present invention, Extraction solvent are ethanol water, will
Extracting solution concentration, drying, obtain selfheal crude extract.
In the step (1) of the present invention, the dosage of Extraction solvent can be 2~30 times of the weight of the selfheal, excellent
Elect 5~25 times as, more preferably 15~22 times.When using water as solvent, extracting method can be selected from decocting method, heat back
Stream method, ultrasonic extraction etc..When using ethanol water as solvent, extracting method can be selected from infusion process, be heated to reflux
Method, ultrasonic extraction, percolation etc., are preferably ultrasonic extraction or percolation.When using heating reflux method or ultrasonic extraction
When, it is preferable that extraction time is 1~4 time, is preferably 1~3 time, more preferably 1~2 time.Preferably, each extraction time is
0.5~4 it is small when, be preferably 1~3 it is small when, more preferably 1~2 it is small when.
It should be noted that in step (1), when being used as Extraction solvent using ethanol water, and extraction time is more than 1
When, the Extraction solvent used every time is not limited to the ethanol water of same concentrations, can be any dense in the scope of the invention
The ethanol water of degree.
In the step (1) of the present invention, the Extraction solvent can be water, and in step (2), the 3rd eluant, eluent can be
Concentration of alcohol is the ethanol water of 50~60vol%；Or Extraction solvent described in step (1) can be ethanol water,
3rd eluant, eluent described in step (2) can be the ethanol water that concentration of alcohol is 65~75vol%.In step (1)
The concentration of ethanol water can be 20~95vol%, be preferably the ethanol water of 50~80vol%, further preferably for 60~
The ethanol water of 70vol%.
In the step (2) of the present invention, using water as dispersant, sample solution is made in the selfheal crude extract, and will
The sample solution is placed in macroporous resin column；Wherein, the selfheal crude extract content in the sample solution is 10~50g/100ml.
In the present invention, selfheal crude extract content is preferably 20~40g/100ml, more preferably 25~35g/100ml；Step (2)
The water used is preferably distilled water, deionized water etc..Macroporous resin column is preferably using the tree of the separation of suitable low pole material, purifying
Fat, such as AB-8 macroreticular resins, D-101 types macroporous absorbent resin, D-101-I type macroporous absorbent resins etc., are preferably AB-8 big
Hole resin.
In the step (2) of the present invention, after sample solution loading, successively using the first eluant, eluent, the second eluant, eluent and the
Three eluant, eluents carry out gradient elution, respectively obtain the first eluent, the second eluent and the 3rd eluent.3rd eluant, eluent is washed
Eluent concentration, the drying obtained after de-, obtains the Prunella vulgaris extract of the present invention.A specific embodiment party according to the present invention
Formula, the first eluant, eluent are water, its dosage is 1~4 times of the volume of the sample solution, is preferably 1~3 times, more preferably 1.5~
2.5 again；Second eluant, eluent is the ethanol water that concentration of alcohol is 10~30vol%, more preferably the ethanol of 15~25vol%
Aqueous solution, its dosage are 1~4 times of the volume of the sample solution, are preferably 2~4 times, more preferably 2.5~3.5 times；3rd
Eluant, eluent is the ethanol water that concentration of alcohol is 50~95vol%, is preferably the ethanol water of 50~75vol%, it is used
Measure the volume for the sample solution 1~10 times, is preferably 2~8 times, more preferably 4~7 times, more preferably 4~6 times.
In the step (2) of the present invention, the 3rd eluant, eluent can once be eluted, and time can also wash at twice or more
It is de-, such as the ethanol water of the 3rd eluant, eluent ethanol water and 95vol% that are adopted as 50vol% successively eluted,
Obtain the 3rd eluent.
In the step (3) of the present invention, the 3rd eluent is concentrated, it is dry, obtain the Prunella vulgaris extract of the present invention.Institute
Stating concentration and drying means can use this area conventional method to operate, and which is not described herein again.
A preferred embodiment according to the present invention, the Prunella vulgaris extract obtain as follows：
(1) selfheal is extracted by the use of water as Extraction solvent, obtains selfheal crude extract；Extracting method for heating reflux method or
Ultrasonic extraction, extraction time are 1~3 time, and when each extraction time is 1~2 small, the dosage of each Extraction solvent is selfheal
5~25 times of weight；
(2) the selfheal crude extract is placed in macroporous resin column, successively using the first eluant, eluent, the second eluant, eluent and
Three eluant, eluents carry out gradient elution, collect the eluent after the 3rd eluent；First eluant, eluent is water, its dosage is
1.5~2.5 times of the volume of the sample solution；Second eluant, eluent is that the ethanol that concentration of alcohol is 15~25vol% is water-soluble
Liquid, its dosage are 2~4 times of the volume of the sample solution；3rd eluant, eluent is the second that concentration of alcohol is 50~60vol%
Alcohol solution, its dosage are 4~7 times of the volume of the sample solution；
(3) by eluent concentration, the drying after the 3rd eluent, Prunella vulgaris extract is obtained.
Another preferred embodiment according to the present invention, the Prunella vulgaris extract obtain as follows：
(1) selfheal is extracted as Extraction solvent by the use of the ethanol water that concentration of alcohol is 50~80vol%, it is withered obtains the summer
Careless crude extract；Extracting method is ultrasonic extraction or heating and refluxing extraction, and extraction time is 1~3 time, and each extraction time is 1~2
Hour, the dosage of each Extraction solvent is 5~25 times of the weight of selfheal；
(2) the selfheal crude extract is placed in macroporous resin column, successively using the first eluant, eluent, the second eluant, eluent and
Three eluant, eluents carry out gradient elution, collect the eluent after the 3rd eluent；First eluant, eluent is water, its dosage is
1.5~2.5 times of the volume of the sample solution；Second eluant, eluent is that the ethanol that concentration of alcohol is 15~25vol% is water-soluble
Liquid, its dosage are 2~4 times of the volume of the sample solution；3rd eluant, eluent is the second that concentration of alcohol is 65~75vol%
Alcohol solution, its dosage are 4~7 times of the volume of the sample solution；
(3) by eluent concentration, the drying after the 3rd eluent, Prunella vulgaris extract is obtained.
In the dripping pill of the present invention, the matrix can use the dripping pill matrix of this area routine.It is preferably, of the invention
Matrix can be selected from polyethylene glycol (PEG), polyoxyl 40 stearate (S-40), odium stearate, glycerin gelatine, urea,
Poloxamer etc..Preferred embodiment according to the present invention, the matrix are polyethylene glycol, more preferably polyethylene glycol-6000
And/or polyethylene glycol-4000.
An embodiment according to the present invention, the dripping pill of the invention containing Prunella vulgaris extract include：
5~20 parts by weight of Prunella vulgaris extract,
20~60 parts by weight of polyethylene glycol-6000, and
10~40 parts by weight of polyethylene glycol-4000.
Preferably, the dripping pill containing Prunella vulgaris extract includes：
5~20 parts by weight of Prunella vulgaris extract,
20~45 parts by weight of polyethylene glycol-6000, and
10~30 parts by weight of polyethylene glycol-4000.
It is highly preferred that the dripping pill containing Prunella vulgaris extract includes：
10~20 parts by weight of Prunella vulgaris extract,
20~45 parts by weight of polyethylene glycol-6000, and
10~30 parts by weight of polyethylene glycol-4000.
In the present invention, it is preferable that the dripping pill containing Prunella vulgaris extract only contains said components.
A preferred embodiment according to the present invention, the dripping pill containing Prunella vulgaris extract include：Prunella vulgaris extract
20 parts by weight, 20 parts by weight of polyethylene glycol-6000, and 20 parts by weight of polyethylene glycol-4000.
Another preferred embodiment according to the present invention, the dripping pill containing Prunella vulgaris extract include：Selfheal is extracted
15 parts by weight of thing, 20 parts by weight of polyethylene glycol-6000, and 10 parts by weight of polyethylene glycol-4000.
The present invention also provides a kind of preparation method of the dripping pill containing Prunella vulgaris extract, include the following steps：
(A) Prunella vulgaris extract is uniformly mixed with the matrix melted, is made into liquid；
(B) liquid is instilled in condensate liquid by the water dropper of pill dripping machine, so as to solidify to form pellet, removes condensation
Liquid, obtains dripping pill.
According to embodiment of the present invention, can be finely ground by the Prunella vulgaris extract in step (A), excessively 70~
100 mesh sieves, are preferably 80 mesh sieves, add absolute ethyl alcohol dissolving, are then uniformly mixed with the matrix of melting, are stirred at 70~75 DEG C
Ethanol is removed, insulation is stood to bubble-free, obtains the liquid.According to another implementation of the invention, in step (A),
The Prunella vulgaris extract is finely ground, 70~100 mesh sieves are crossed, is preferably 80 mesh sieves, is then uniformly mixed with the matrix of melting, are protected
Temperature is stood to bubble-free, obtains the liquid.The temperature of the matrix of above-mentioned melting is 70~75 DEG C.
In the step (B) of the present invention, fluid temperature (dripping temperature) is 70~80 DEG C, water dropper and condensate liquid liquid level distance
For 6~8cm, condensate temperature is 0~4 DEG C, and drop speed is 20~40 drops/min, and condensate liquid depth is 35~45cm.The present invention's
The water dropper diameter (inner/outer diameter) of pill dripping machine can be 2.5mm/3.6mm or 3.0mm/4.2mm.According to the present invention one it is excellent
Embodiment is selected, fluid temperature is 70 DEG C, a diameter of 3.0mm/4.2mm of water dropper of pill dripping machine, water dropper and condensate liquid liquid level distance
For 6cm, condensate liquid depth is 35cm.After dripping pill cools down, incline condensate liquid, collects dripping pill, drip is net and is removed with filter paper
Condensate liquid on ball.
The dripping pill that preparation method using the present invention obtains, has good roundness, weight differential small, leaches time limit conjunction
Lattice.The inventors of the present application found that the dripping pill of the present invention has significant sedative-hypnotic effect, clinical test finds that its treatment is lost
Dormancy effect is substantially better than Prunella vulgaris extract made from existing extracting method.In addition, present inventor it has surprisingly been found that with
The preparation of stomach approach administration is compared, and clinically treatment insomnia is total effective for pill of the invention (being administered using sublingual administration)
Rate reaches 100%, and wherein cure rate is up to 93.33%, and has no toxic side effect, while convenient to take, and patient acceptance is high.
Embodiment
The preparation method of the dripping pill containing Prunella vulgaris extract of the present invention, but this are illustratively described by the following examples
The protection domain not limited to this of invention.
Preparation example 1- Prunella vulgaris extracts A
The preparation method of Prunella vulgaris extract of the present invention is：
(1) selfheal is extracted by the use of water as Extraction solvent, heating and refluxing extraction 2 times, every time plus 10 times of amount water extract 1h, close
It is dry and extracting solution, extracting solution are concentrated under reduced pressure, obtain selfheal crude extract.
(2) the selfheal crude extract is scattered in deionized water, it is 31g/100ml to obtain selfheal crude extract content
Sample solution, sample solution is placed in AB-8 macroporous resin columns, successively using the deionized water of 2 times of volumes, 3 times of volumes
20vol% ethanol waters and the 50vol% ethanol waters of 5 times of volumes carry out gradient elution as eluant, eluent.
(3) eluent after the elution of 50vol% ethanol waters is collected, concentration, drying, obtain Prunella vulgaris extract A.
Preparation example 2- Prunella vulgaris extracts B
(1) selfheal, the ultrasonic extraction 2 at 45 DEG C are extracted by the use of 70vol% ethanol waters as Extraction solvent ultrasonic method
Secondary, every time plus 20 times of amount ethanol waters extract 1h, merge extracting solution, are concentrated under reduced pressure into no alcohol taste, dry, and it is thick to obtain selfheal
Extract.
(2) the selfheal crude extract is dispersed in water, obtains the loading that selfheal crude extract content is 31g/100ml
Liquid, AB-8 macroporous resin columns are placed in by sample solution, successively using the 20vol% ethanol of the deionized water of 2 times of volumes, 3 times of volumes
Aqueous solution and the 70vol% ethanol waters of 5 times of volumes carry out gradient elution as eluant, eluent.
(3) eluent after the elution of 70vol% ethanol waters is collected, which is concentrated, it is dry, obtain selfheal
Extract B.
Preparation example 3
(1) selfheal is extracted by the use of water as Extraction solvent, ultrasonic extraction 3 times, 35 DEG C of ultrasonic temperature, every time plus 10 times are measured water
1.5h is extracted, merges extracting solution, extracting solution is concentrated under reduced pressure, dry, obtains selfheal crude extract；
(2) the selfheal crude extract is scattered in deionized water, it is 50g/100ml to obtain selfheal crude extract content
Sample solution, the sample solution is placed in AB-8 macroporous resin columns, successively using the deionized water of 4 times of volumes, 2 times of volumes
15vol% ethanol waters and the 60vol% ethanol waters of 5 times of volumes carry out gradient elution as eluant, eluent；
(3) eluent after the elution of 60vol% ethanol waters is collected, is concentrated, it is dry, obtain Prunella vulgaris extract.
Preparation example 4
(1) Extraction solvent, ultrasonic method extraction selfheal, the ultrasonic extraction 2 at 45 DEG C are used as by the use of 50vol% ethanol waters
Secondary, every time plus 20 times of amount ethanol waters extract 1h, merge extracting solution, are concentrated under reduced pressure into no alcohol taste, dry, and it is thick to obtain selfheal
Extract；
(2) the selfheal crude extract is dispersed in water, obtains the loading that selfheal crude extract content is 20g/100ml
Liquid, AB-8 macroporous resin columns are placed in by the sample solution, successively using the 25vol% of the deionized water of 2 times of volumes, 4 times of volumes
Ethanol water and the 75vol% ethanol waters of 6 times of volumes carry out gradient elution as eluant, eluent；
(3) eluent after the elution of 75vol% ethanol waters is collected, which is concentrated, it is dry, obtain selfheal
Extract.
Preparation example 5
(1) by the use of ethanol water as Extraction solvent, heating and refluxing extraction selfheal 3 times, the ethanol of extraction operation three times
The concentration of aqueous solution is 95vol%, 70vol% and 20vol% respectively, and solubilization dosage is 10 times of selfheal medicinal material respectively three times
Amount, 12 times of amounts, 12 times of amounts, extraction time are 1h, 1h, 1h respectively, merge extracting solution, and extracting solution is concentrated under reduced pressure, dry, obtains the summer
Withered grass crude extract；
(2) the selfheal crude extract is dispersed in water, obtains the loading that selfheal crude extract content is 25g/100ml
Liquid, by AB-8 macroporous resin columns on the sample solution, successively using the deionized water of 3 times of volumes, the 10vol% second of 4 times of volumes
The 90vol% ethanol waters of alcohol solution, the 75vol% ethanol waters of 5 times of volumes and 5 times of volumes as eluant, eluent, into
Row gradient elution；
(3) eluent after the elution of 75vol% ethanol waters is collected respectively, and after the elution of 90vol% ethanol waters
Eluent, the eluent is mixed, is concentrated, it is dry, obtain Prunella vulgaris extract.
Embodiment 1
Prunella vulgaris extract made from the preparation example 1 of 20 parts by weight is finely ground, 80 mesh sieves are crossed, add absolute ethyl alcohol dissolving.
The polyethylene glycol-4000 of the polyethylene glycol-6000 of 20 parts by weight of matrix and 20 parts by weight is melted under 70 DEG C of heating water baths.So
The ethanol solution of Prunella vulgaris extract is uniformly mixed with the matrix melted afterwards, stirring removing ethanol at 70 DEG C, insulation standing is extremely
Bubble-free, obtains liquid.Gained liquid is added into pill dripping machine, dripping temperature is 70 DEG C, a diameter of 3.0mm/ of water dropper of pill dripping machine
4.2mm, water dropper are 6cm with condensate liquid liquid level distance, and condensate temperature is 4 DEG C, and drop speed is 20 drops/min, and condensate liquid depth is
35cm.After cooling, incline condensate liquid, and drip is net and removes condensate liquid on ball with filter paper, obtains dripping pill.
Embodiment 2
Prunella vulgaris extract made from the preparation example 2 of 15 parts by weight is finely ground, cross 80 mesh sieves.By the poly- of 20 parts by weight of matrix
The polyethylene glycol-4000 of ethylene glycol -6000 and 10 parts by weight melts under 75 DEG C of heating water baths.Then by Prunella vulgaris extract with
The matrix of melting is uniformly mixed, and stirring removing ethanol at 75 DEG C, insulation standing obtains liquid to bubble-free.Gained liquid is added
Enter pill dripping machine, dripping temperature is 75 DEG C, a diameter of 3.0mm/4.2mm of water dropper of pill dripping machine, and water dropper is with condensate liquid liquid level distance
8cm, condensate temperature are 0 DEG C, and drop speed is 40 drops/min, and condensate liquid depth is 45cm.After cooling, incline condensate liquid, drip
Only condensate liquid on ball is removed and with filter paper, obtains dripping pill.
Embodiment 3
Except " Prunella vulgaris extract made from preparation example 1 " in embodiment 1 is replaced with " selfheal made from preparation example 4
Extract ", other steps and condition are same as Example 1, and dripping pill is prepared.
Embodiment 4
Specific formula is as follows：Prunella vulgaris extract made from the preparation example 5 of 20 parts by weight, the polyethylene glycol of 45 parts by weight-
The polyethylene glycol-4000 of 6000,30 parts by weight；Remaining step and condition are same as Example 2, and dripping pill is prepared.
The drug effect of the Prunella vulgaris extract of the present invention is verified below by way of pharmacological evaluation and clinical trial.
<Experimental animal, material and instrument>
In following experimental example, the mouse used is healthy kunming mice, LAF/SPF ranks, 30~40g of weight, by Beijing
Tie up experimental animal Technology Co., Ltd. of tonneau China to provide, licensing numbering：SCXK (capital) 2015-000.Experimental situation is：Temperature
24 ± 0.5 DEG C, humidity is maintained at 60 ± 2%, and indoor light control is free in normal circadian rhythm (bright light during morning 8), animal
Obtain food and water.
The Prunella vulgaris extract A used in following experimental example is obtained by embodiment 1；Prunella vulgaris extract B is logical
Cross the product of the acquisition of embodiment 2.
Mouse automatic movable analysis system：Using 30cm × 30cm × 40cm cartons, internal blacking, sieve skill (Logitech)
C920 high-definition cameras (12,000,000 pixel) record mouse activity, using DigBehv animal behaviors analysis system 2.0, Shang Haiji
Measure software Science and Technology Ltd..
<The experimental study of Prunella vulgaris extract tranquilizing soporific drug effect>
Test influence of the Prunella vulgaris extract to mouse autonomic activities
1 experiment material
1.1 animal：Healthy kunming mice.
1.2 medicine：Prunella vulgaris extract A and Prunella vulgaris extract B, respectively plus water is configured to 0.14g/ml；It is stable：
0.3g/ml。
1.3 instrument：Mouse autonomic activities analysis system.
2 experimental methods
2.1 packet：4 groups are randomly divided into, every group 10, is followed successively by deionized water group, stable group, Prunella vulgaris extract A groups
(A groups hereinafter referred to as of the present invention), Prunella vulgaris extract B groups (B groups hereinafter referred to as of the present invention).
2.2 administration：It is intraperitoneal injection medicine, dosage is shown in Table 1.
1 dosage of table
2.3 method：Mouse is put into the case of autonomic activities field before administration, after adapting to 3min, the continuous 5min that records independently lives
Dynamic video, 20min after intraperitoneal injection, the same method, records mouse autonomic activities 5min again, and is divided by software
Analysis.
3 experimental results
Mouse autonomic activities total distance is shown in Table 2.The total distance no significant difference before each group administration.After administration, with
Deionized water group compares, and stable group and A groups of the present invention, the mouse autonomic activities total distance of B groups of the present invention substantially reduce.
2 mouse autonomic activities total distance of table
* represents to compare with deionized water group, P ＜ 0.01
The mouse autonomic activities time is shown in Table 3.The activity time no significant difference before each group administration.After administration, with
Deionized water group compares, and stable group and A groups of the present invention, the mouse autonomic activities time of B groups of the present invention substantially reduce.
The 3 mouse autonomic activities time of table
* represents to compare with deionized water group, P ＜ 0.01
Testing two Prunella vulgaris extracts influences sub-threshold dose pentobarbital sodium in mice sleep number of elements
1 experiment material
1.1 animal：Healthy kunming mice.
1.2 medicine：Prunella vulgaris extract A and Prunella vulgaris extract B, respectively plus water is configured to 0.14g/ml；It is stable：
0.3g/ml；Yellow Jackets：1.8mg/ml.
1.3 instrument：Mouse autonomic activities analysis system.
2 experimental methods
2.1 packet：4 groups are randomly divided into, every group 13, is followed successively by deionized water group, stable group, Prunella vulgaris extract A groups
(A groups hereinafter referred to as of the present invention), Prunella vulgaris extract B groups (B groups hereinafter referred to as of the present invention).
2.2 administration：It is intraperitoneal injection medicine.
2.3 method：30min after administration, intraperitoneal injection sub-threshold dose yellow Jackets (18mg/kg), record mouse right
Areflexia and recovery time, righting reflex loss ＞ 1min are denoted as sleep.
3 experimental results
Sub-threshold dose pentobarbital sodium in mice sleep situation the results are shown in Table 4.
4 sub-threshold dose pentobarbital sodium in mice sleep situation (n=13) of table
* represents to compare with deionized water group, P ＜ 0.01
Test influence of three Prunella vulgaris extracts to mouse autonomic activities
1 experiment material
1.1 animal：Healthy kunming mice.
1.2 medicine：Prunella vulgaris extract A and Prunella vulgaris extract B, respectively plus water is configured to 0.14g/ml；It is stable：
0.3g/ml；Yellow Jackets：1.8mg/ml.
1.3 instrument：Mouse autonomic activities analysis system.
2 experimental methods
2.1 packet：4 groups are randomly divided into, every group 10, is followed successively by deionized water group, stable group, Prunella vulgaris extract A groups
(A groups referred to as of the present invention), Prunella vulgaris extract B groups (B groups referred to as of the present invention).
2.2 administration：It is intraperitoneal injection, dosage is shown in Table 5.
5 dosage of table
2.3 method：Mouse is put into the case of autonomic activities field before administration, after adapting to 3min, the continuous 5min that records independently lives
Dynamic video.Mouse, is put into a case by 20min after intraperitoneal injection again, the same method, records mouse autonomic activities 5min,
And analyzed by software.
3 experimental results
Mouse autonomic activities total distance is shown in Table 6.The total distance no significant difference before each group administration.After administration, with
Deionized water group compares, and stable group and A groups of the present invention, the mouse autonomic activities total distance of B groups of the present invention substantially reduce.
6 mouse autonomic activities total distance of table
* represents to compare with deionized water group, * * P ＜ 0.01, * P ＜ 0.05
The mouse autonomic activities time is shown in Table 7.The activity time no significant difference before each group administration.After administration, with
Deionized water group compares, and stable group and A groups of the present invention, the mouse autonomic activities total distance of B groups of the present invention substantially reduce.
The 7 mouse autonomic activities time of table
* represent compared with deionized water group, P ＜ 0.01.
<Selfheal dripping pill effect for the treatment of insomnia clinical and experimental study>
Selfheal dripping pill is prepared according to the method for embodiment 1, medicine 5mg is carried per grain ball, equivalent to selfheal
Crude drug absolute dosage 5g.Selfheal granule is packaged into every bag of 1.5g, every bag of corresponding selfheal crude drug purchased from benevolence doctor's hall
30g。
1 clinical data
1.1 general information
Receive the insomniac 30 for the treatment of during collecting in October, 2015~2016 year April, be randomly divided into two groups：
Dripping pill group 15, man 7, female 8,26~65 years old age；
Particle group 15, man 6, female 9, the age was at 22~59 years old.
Two groups of courses of disease are most 3 months short, most 22 years long.Two groups of data are statistically analyzed that there was no significant difference (P>0.05),
It is comparable.
1.2 diagnostic criteria
Reference《Spirit and the clinical description of behavior disorder classification and diagnostic point (ICD-10)》On nonorganic insomnia
Diagnostic criteria：
(1) difficulty falling asleep, or be difficult to maintain sleep, or poor sleeping quality；
(2) it is sleep disordered at least to occur 3 times weekly and continue more than 1 month；
(3) day and night it is absorbed in insomnia, the consequence of excessive worry insomnia；
(4) amount of sleep and the dissatisfied of matter cause obvious worries, or have impact on society and occupational function.
Referring concurrently to tcm diagnosis reference《Chinese medical disease Standardization of diagnosis and curative effect》：
(1) the lighter's difficulty of falling asleep or sleep but easy to wake, are insomnia, severe one is lain awake all night after waking up.
(2) diseases such as headache, giddy, palpitaition, forgetful, dreaminess are often accompanied by.
(3) it is no abnormal through each system and laboratory examination.
1.3 criterion of therapeutical effect
Reference《Mental illness therapeutic effect standard trim draft》：
Recovery from illness：It is deeply, energetic after waking up in more than 6h, sleep that the length of one's sleep recovers the normal or length of one's sleep.
It is effective：Sleep is clearly better, and sleeps in more than 3h.
Effectively：The length of one's sleep substantially increases before relatively treating, but less than 3h.
It is invalid：Insomnia is without improvement after treatment.
2 treatment methods
2.1 selfheal dripping pill groups
Patient sleeps preceding 30 minutes sublingual administrations 6 daily, equivalent to intake selfheal crude drug 30g, daily medication 1 time,
Continuously take 7 days, medication next day get up after fill in Sleep questionnaire questionnaire.
2.2 selfheal particle groups
Patient sleeps first 30 minutes daily to take after mixing it with water 1 bag, and daily medication 1 time, continuously takes 7 days, medication next day get up after fill in
Sleep questionnaire questionnaire.
3 results
Toxic side effect is showed no in two groups of therapeutic processes, efficacy result is shown in Table 8.
8 two groups of curative effects of table compare
| Group | N | Recovery from illness | It is effective | Effectively | It is invalid | Total effective rate |
| Dripping pill group | 15 | 14 | 1 | 0 | 0 | 100%* |
| Particle group | 15 | 7 | 3 | 1 | 4 | 73.3% |
Compared with particle group, * P<0.05
Present invention is not limited to the embodiments described above, in the case of without departing substantially from the substantive content of the present invention, this area skill
Any deformation, improvement, the replacement that art personnel are contemplated that each fall within the scope of the present invention.
Claims (10)
1. a kind of dripping pill containing Prunella vulgaris extract, it is characterised in that the dripping pill includes Prunella vulgaris extract and matrix；Its
In, the Prunella vulgaris extract obtains as follows：
(1) selfheal is extracted as Extraction solvent by the use of water or ethanol water, obtains selfheal crude extract, the ethanol water
In concentration of alcohol be 20~95vol%；
(2) the selfheal crude extract is placed in macroporous resin column, is washed successively using the first eluant, eluent, the second eluant, eluent and the 3rd
De- agent carries out gradient elution, collects the eluent after the 3rd eluent；First eluant, eluent is water, second elution
Agent is the ethanol water that concentration of alcohol is 10~30vol%, and the 3rd eluant, eluent is that concentration of alcohol is 50~95vol%
Ethanol water；
(3) by eluent concentration, the drying after the 3rd eluent, Prunella vulgaris extract is obtained.
2. dripping pill according to claim 1, it is characterised in that：
In step (1), the Extraction solvent is water；In step (2), the 3rd eluant, eluent is concentration of alcohol for 50~
The ethanol water of 60vol%；Or
Extraction solvent described in step (1) is ethanol water, the 3rd eluant, eluent described in step (2) is concentration of alcohol for 65~
The ethanol water of 75vol%.
3. dripping pill according to claim 1, it is characterised in that using water as dispersant, the summer is withered in step (2)
Sample solution is made in careless crude extract, and the sample solution is placed in macroporous resin column；Wherein, the selfheal in the sample solution slightly carries
Thing content is 10~50g/100ml.
4. dripping pill according to claim 3, it is characterised in that the Prunella vulgaris extract is obtained by following specific steps
：
(1) selfheal is extracted by the use of water as Extraction solvent, obtains selfheal crude extract；Extracting method is heating reflux method or ultrasound
Extraction method, extraction time are 1~3 time, and when each extraction time is 1~2 small, the dosage of each Extraction solvent is the weight of selfheal
5~25 times of amount；
(2) the selfheal crude extract is placed in macroporous resin column, is washed successively using the first eluant, eluent, the second eluant, eluent and the 3rd
De- agent carries out gradient elution, collects the eluent after the 3rd eluent；First eluant, eluent is water, its dosage is described
1.5~2.5 times of the volume of sample solution；Second eluant, eluent is the ethanol water that concentration of alcohol is 15~25vol%, its
Dosage is 2~4 times of the volume of the sample solution；3rd eluant, eluent is the ethanol water that concentration of alcohol is 50~60vol%
Solution, its dosage are 4~7 times of the volume of the sample solution；
(3) by eluent concentration, the drying after the 3rd eluent, Prunella vulgaris extract is obtained.
5. dripping pill according to claim 3, it is characterised in that the Prunella vulgaris extract is obtained by following specific steps
：
(1) selfheal is extracted as Extraction solvent by the use of the ethanol water that concentration of alcohol is 50~80vol%, it is thick obtains selfheal
Extract；Extracting method is ultrasonic extraction or heating and refluxing extraction, and extraction time is 1~3 time, and each extraction time is small for 1~2
When, the dosage of each Extraction solvent is 5~25 times of the weight of selfheal；
(2) the selfheal crude extract is placed in macroporous resin column, is washed successively using the first eluant, eluent, the second eluant, eluent and the 3rd
De- agent carries out gradient elution, collects the eluent after the 3rd eluent；First eluant, eluent is water, its dosage is described
1.5~2.5 times of the volume of sample solution；Second eluant, eluent is the ethanol water that concentration of alcohol is 15~25vol%, its
Dosage is 2~4 times of the volume of the sample solution；3rd eluant, eluent is the ethanol water that concentration of alcohol is 65~75vol%
Solution, its dosage are 4~7 times of the volume of the sample solution；
(3) by eluent concentration, the drying after the 3rd eluent, Prunella vulgaris extract is obtained.
6. dripping pill according to claim 1, it is characterised in that it is stearic that the matrix is selected from polyethylene glycol, polyoxyethylene list
Acid esters, odium stearate, glycerin gelatine, urea or poloxamer.
7. dripping pill according to claim 1, it is characterised in that the dripping pill includes：
5~20 parts by weight of Prunella vulgaris extract,
20~60 parts by weight of polyethylene glycol-6000, and
10~40 parts by weight of polyethylene glycol-4000.
8. according to the preparation method of claim 1~7 any one of them dripping pill, it is characterised in that the preparation method includes
Following steps：
(A) Prunella vulgaris extract is uniformly mixed with the matrix melted, is made into liquid；
(B) liquid is instilled in condensate liquid by the water dropper of pill dripping machine, so as to solidify to form pellet, removes condensate liquid, obtain
To dripping pill.
9. preparation method according to claim 8, it is characterised in that
It is in step (A), the Prunella vulgaris extract is finely ground, 70~100 mesh sieves are crossed, absolute ethyl alcohol dissolving are added, with melting
Matrix is uniformly mixed, and stirring removing ethanol at 70~75 DEG C, insulation standing obtains the liquid to bubble-free；Or
It is in step (A), the Prunella vulgaris extract is finely ground, 70~100 mesh sieves are crossed, are uniformly mixed with the matrix of melting, are kept the temperature
Stand to bubble-free, obtain the liquid.
10. preparation method according to claim 8, it is characterised in that
In step (B), fluid temperature is 70~80 DEG C, and water dropper and condensate liquid liquid level distance be 6~8cm, condensate temperature is 0~
4 DEG C, drop speed is 20~40 drops/min, and condensate liquid depth is 35~45cm.
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